Solvent dyeing or solvent creaseproofing with steam and solvent vapor drying

ABSTRACT

A process for the application of a finishing agent to a substrate which comprises treating the substrate with a solution, or a dispersion, or an emulsion of the finishing agent in an organic solvent and then treating the substrate with steam for a time sufficient to remove a major proportion of the organic solvent, and subsequently finally treating the substrate with superheated steam or with the vapor of an organic solvent.

Field of Search 8/94, 174, 175, 116.2, 8/1491; 117/1395 United States Patent 1 1111 3,784,355

Fielding Jan. 8, 1974 SOLVENT DYEING OR SOLVENT [56] References Cited CREASEPROOFING WITH STEAM AND UNITED S T N S SOLVENT VAPOR DRYING 1,859,084 5/1932 Gore 195/64 x [75 Inventor; Brian C i Fielding, R 3,523,749 8/1970 MacLeod et a1 8/94 X g England OTHER PUBLICATIONS Assignee: Imperial Chemical Industries Whites American Dyestuff Reporter, July '3, 1967,

1 Limited, London, England page 59 597 [22] Filed: Nov. 8, 1971 Primary ExaminerDona1d Levy [2]] Appl AttorneyCushman, Darby & Cushman [30] Foreign Application Priority Data 57 ABSTRACT Nov. 6, 1970 Great Britain 52943/70 A process for the application of a finishing agent to a substrate which comprises treating the substrate with a {52] U.S.I Cl 8/175, 8/176, 8/184, Solution or a dispersion, or an emulsion of the finish 8/186 8/14 S/DIG' 8/1491 17/1395 ing agent in an organic solvent and then treating the 1 17/335 1 17/1394 I 17/155 I 17/]29'5A substrate with steam for a time sufficient to remove :1

117/155 8/150 major proportion of the organic solvent, and subse- [51 Int. Cl 006p /02 quenfly finally treating the Substrate with superheated [58] steam or with the vapor of an organic solvent.

10 Claims, No Drawings SOLVENT DYEING R SOLVENT CREASEPROOFING WITH STEAM AND SOLVENT VAPOR DRYING This invention relates to the application of finishing agents, and mare particularly to the application of fin ishing agents which impart specific properties, for example crease-resistance, water-repellency and/or resistance to soiling to substrates such as textile materials, paper or plastics.

In lim t in sm Pi sp s t fi-- ll Q there is described and cl aimed a process for the application of a finishing agent to a substrate which comprises treating the substrate with a solution, or a dispersion, or an emulsion of the finishing agent in an organic solvent and then treating the substrate with steam for a time sufficient to remove a major proportionof the organic solvent.

lnsaid United Kingdom Patent Specification there is described also, following the operation of removing the solvent from the treated materials, a further step in which the finishing agent is fixed to the substrate by means of heating at a higher temperature than that attained in the steam treatment zone, for example by means of conventional heating equipment such as drying cylinders, a baking oven (i.e., hot-air at about 140 to 160 C) or a stenter.

We have now found that good, and in some cases improved, results are obtained in the process described and claimed in United Kingdom Pat. specification No. 1,175,208 if the step to which the treated material is subjected to fix the finishing agent to the substrate comprises subjecting the treated material to a treatment with the vapour of an organic solvent or with superheated steam.

According to the present invention, therefore, we provide a process for the application of a finishing agent to a substrate which comprisestreating the substratewith a solution, or a dispersion, or an emulsion of the finishing agent in an organic solvent and then treating the substrate with steam to remove a major portion of the organic solvent, and subsequently finally treating the substrate with superheated steam or with the vapour of an organic solvent. The temperature of the superheated solvent vapour should be equal to or greater than the boiling point of said solvent.

After removal of a major proportion and preferably substantially all of the organic solvent used to apply the finishing agent to the substrate, the substrate is treated with solvent vapour or with super-heated steam. In the above case where superheated steam is employed this will usually be at a temperature which is at least 120 C and may be, for example, up to 200 C; we prefer to employ the steam at a temperature of about 130 to 160 C for most practical purposes. The superheated steam may be heated to the desired high temperature prior to its entry into the treatment vessel orit may be heated within the vessel, for example by means of electric heaters or infra-red heaters located within the vessel, which normally will be lagged to minimise heat losses therefrom. Any traces of solvent present in the substrate on entry into the high temperaturesteaming vessel will be removed in the vessel and provision may bemade forrecoverin g the resulting solrecovered in conventional manner. Normally the solvent employed in vapour form for heating the textile material will be the same as the solvent in which the finishing agent was applied to the textile material.

The treatment with superheated steam or solvent vapour normally will be from 30 seconds to 5 minutes. The finishing agents which may be employed in the process and the substrates to which they may be applied are described in detail in United Kingdom Pat.

specification No. 1,175,208 in which also are described in detail suitable techniques and conditions for applying the finishing agents to the substrate and for removing the organic solvent by treatment of the substrate with steam.

The steam used to remove the solvent after application of the finishing agent may contain a proportion of water and we have found that steam at a pressure of from 10 to 30 and preferably between 14 and 16 lbs/square inch absolute in equilibrium with liquid water may conveniently be used. The temperature during this treatment with steam should be above the boiling point of the organic solvent or of any azeotrope formed by the solvent and water, and normally will be from to C.

Clearly the choice of the organic solvent used to apply the finishing agent depends upon the nature of the finishing agent to be applied, but there are several other important considerations; for example it is necessary to employ a solvent that does not have any deleterious effect on the textile material or on associated chemical entities such as dyestuffs. Furthermore it is highly desirable that the solvent should be nonflammable and sufficiently volatile to be capable of being removed rapidly from the textile material. We have found that halogenated (particularly chlorinated) hydrocarbon solvents, for example halogenated aliphatic hydrocarbon solvents such as trichloroethylene,

perchloroethylene, 1 ,1,l-tr1chloroethane, methylene chloride, 1,1,2-trichloro-1,2,2-trifluoroethane or mixtures thereof may be employed successfully in our process in the application of finishing agents to textile .mateials. Such finishing agents include agents imparting crease-resistance, shrink-resistance or antistatic properties to the textile material, agents imparting water, dirt-, oilor stain-repellency to the textile material, dyestuffs and fluorescent brighteners.

We have found that the steam treatment time for removal of the solvent is dependent on the type of material to be treated, on the steam temperature and pres sure, on the boiling point of the solvent or of the azeotrope of the solvent and water and on the rate of flow of steam over the material, but that in general a treatment time of from about 2 to 30 seconds is sufficient to remove substantially all (e.g. more than 97 percent 57 weight) of the solvent from the treated materials.

The finishing agent may be applied to the textile material by any conventional means, e.g. impregnating,

doctoring, licking, immersion or spraying, and the steam also may be applied to the textile material in known manner, for example by the method more fully described in UK. Pat. specification No. 916,338, preferably with the modification that the liquid inlet seal to the steam chamber is replaced by a dry seal. Preferably, a method and an apparatus may be used in which the fabric is removed from the steam chamber directly into the atmosphere through a dry seal, as is more fully described in UK. Pat. specification No. 1,170,783. If desired circulation of the steam in the treatment vessel may be assisted by conventional means, e.g. fans, pumps or suction slots.

The process may with advantage be carried out in such a way that the solvent is recovered for re-use after its removal from the textile material. Recovery may be by any conventional method, for example by condensation of the vapours in a condenser positioned inside or outside the flash-off vessel, the condensate being passed to a water separator for removal of any water from the liquid solvent. In this way loss of solvent vapour to the atmosphere can be substantially obviated and the resulting liquid solvent may be re-used.

Treatment of the textile material with steam to remove solvent therefrom and then with superheated steam or solvent vapour can be carried out in separate treatment vessels or alternatively there may be employed a single treatment vessel in which is provided a baffle defining a chamber for the treatment with steam to remove solvent from the textile material and a chamber for the treatment with superheated steam or solvent vapour. Preferably a slight flow of steam or solvent vapour is created from the high temperature chamber to the low temperature chamber.

Particular uses of the invention in which finishing agents are applied to textile materials include the following:

a. A process for treatment of textile materials, especially materials made wholly or in part of cellulosic fibres, by applying thereto a crease-resist resin, particularly crease-resist resins as described in detail in U.K. Pat. specification No. 1,204,163, for example methylated dimethoxy urea resins; these resins may be used togehter with other finishing agents.

b. A process for the shrink-proofing of wool by applying thereto a terpolymer of ethylene, vinyl acetate and methacryloyl chloride.

c. A process for treatment of a substrate by applying thereto a highly fiuorinated organic compound capable of imparting water-, oil-, dirtor stainrepellency to the substrate.

(1. A process for treatment of a substrate by applying thereto a silicone capable of imparting waterrepellency to the substrate.

e. A process for the treatment of textile materials to confer water-repellency thereon by applying thereto a methylolamide of a fatty acid containing at least 14 carbon atoms in the molecule, the said methylolamide cotnaining less than 4.0 percent and preferably less than 2.0 percent by weight of free fatty acids, together with an acid or acidgenerating substance as catalyst.

f. A process for the treatment of textile materials composed wholly or in part of synthetic polymeric material by applying thereto a fluorescent brightening agent of the formula:

wherein A represents a polycyclic aromatic group containing at least three condensed rings, R represents a chloro, substituted amino, alkoxy, substituted alkoxy, aryloxy, alkylthio or substituted alkylthio group, and R2 represents a substituted amino, alkoxy, substituted alkoxy, alkylthio or substituted alkylthio group.

g. A process for the surface modifying ofshapedarti cles composed at least in part of a synthetic, essentially linear crystallisable polyester material by applying to the surface of the shaped article a crystallisable polymeric compound which contains within a single molecule sufficient repeat units identical with those forming the crystallisable portions of the polyester to confer crystallisability on the compound, and at least one active group as hereinafter defined serving to modify the surface of the shaped article.

The substrate to be treated by the process of the invention may be a shaped article of any suitable form or structure and may be made of any suitable material, for example plastic or paper. However our invention finds its main application in the treatment of textile materials, and in particular textile materials which have not been made up into garments, for example fibres, piece goods and other unmade-up textile materials in the woven, knitted, felted or yarn forms. It is in relation to the treatment of textile materials, therefore, that our invention is particularly described. Our invention may be used with particular advantage in the treatment of textile materials to impart creaseresistance and minimum-care properties thereto.

We have found, surprisingly, that textile materials containing cellulosic fibres treated with crease-resist resins by the process of the invention have a better balance of properties, for example wet-crease recovery, tensile strength and abrasion resistance, than textile materials treated similarly but employing hot-air instead of superheated steam or solvent vapour in the resin fixation step. Moreover, good dry-crease recovery is retained.

The invention is illustrated but in no way limited by the following Examples in which all parts are parts by weight:

EXAMPLES l to 6 Five parts of a methylated dimethoxy ethylene urea resin and 1.5 parts of MgCl -6l-l O (as a dispersion in 10 parts of trichloroethylene) were added to parts of trichloroethylene. A mercerised cotton poplin fabric was impregnated with the mixture. The impregnated fabric was then squeezed (pad mangle) such that the amount of the mixture remaining in the fabric was 80 percent by weight based on the dry weight of the fabric. The fabric was then treated as follows:

Example 1 A sample of fabric was steamed for 30 seconds in steam at about C to remove substantially all the trichloroethylene, and was then heated to C for three minutes in superheated steam. Example 2 A sample of fabric was heated in a hotair oven at about 100 C for 45 seconds to remove substantially all the trichloroethylene, and was then heated to 155 C for 3 minutes in superheated steam.

Example 3 A sample of the fabric was steamed for 30 seconds at about 100 C and was then immersed for 3 minutes in trichloroethylene vapour at about 87 C.

Example 4 A sample of the fabric was heated in a hot-air oven at about 100 C for 45 seconds, and was then immersed for 3 minutes in trichloroethylene vapour at 87 C.

Example 5 A mixture was prepared as described above but using five parts of an alkoxylated propylene urea resin instead of the methylated dimethoxy ethylene urea resin. The fabric was squeezed to 8.0 percent pick-up. The fabric was steamed for 30 seconds at about 100 C, and was then immersed for 3 minutes in perchloroethylene vapour at 122 C.

Example 6 For purposes of comparison a sample of the fabric was steamed for 30 seconds at about 100 C and was then heated in a hot-air oven at 155 C for 3 minutes.

In each example the following properties of the final treated fabric were determined:

Dry-crease recovery angle (warp and weft) D.C.R.

Wet-crease recovery angle 7 (warp '7 and 'iiift" W.C.R.

Ring wear abrasion resistance (revolutions) Abra- Tensile strength (1 inch grap) weft (lbs) T8.

The results are shown in the Table:

ric was impregnated with the resulting white emulsion and was then squeezed on a pad mangle such that the amount of the mixture remaining on the fabric was 90 percent by weight based on the dry weight of the fabric. The fabric was then steamed for 30 seconds in steam at about 100C to remove substantially all the perchloroethylene, and the fabric was then heated to 145 C for 3 minutes in superheated steam.

The treated fabric possessed the following properties:

Dry-crease recovery (warp and weft) 260 Wet-crease recovery (warp and weft) 220 Martindale Abrasion resistance 10,000 rubs Durable-press rating after five washes 3.0 (60 C spin/line dry) EXAMPLE 8 2.2 parts of a self-emulsifying fluorinated polymer available under the trade name Zepel TE were mixed by stirring with 12 parts of trichloroethylene and to this mixture was added, with stirring, 8.9 parts of a melamine-based resin precondensate available as Calaroc MB, 0.45 parts of an amine hydrochloride available as Catalyst AC, 4.5 parts of water and 1.1 part of a catalyst available as Zepel catalyst. The resulting emulsion was diluted with 70.8 parts of trichloroethylene, with vigorous stirring.

A dyed polyester/cotton fabric was impregnated with the resulting emulsion and squeezed on a pad mangle such that the amount of the mixture remaining on the fabric was 90 percent by weight based on the dry weight of the fabric. The fabric was then steamed for 30 seconds in steam at about 100 C to remove substantially all the trichloroethylene, and the fabric was then immersed for 2 minutes in trichloroethylene vapour at about 87 C.

The final treated fabric possessed the following properties:

The 'Control is the untreated 'f a'bi'ie'.

D.C.R. 229

W.C.R. 235 Abrasion 2,300 T.S. 38

EXAMPLE 7 19 parts of a water-soluble methylated urea resin available under the trade name Knittex LDl-l, 1.9

parts of an inorganic metal salt catalyst available underthe trade name Catalyst Z58, 5.5 parts of water and 1.1 parts of an oxyethylenated emulsifying agent (anionic) available under the trade name Oleanat L-EM were mixed together, with stirring, and the resulting paste was stirred slowly into 72.5 parts of perchloroethylene. A cotton/regenerated cellulose (Vincel) fab- Treat e721 I Untreated fiabric fabric Dry-crease recovery (warp and weft) 305 245 Wet-crease recovery (warp and weft) 290 230 After one wash at 60 C and line drying, the treated fabric had a Spray Rating of and Oil Repellency Rating of 7 compared with 0 and less than 1 respectively for the untreated fabric.

What we claim is:

1. A process for the application of a finishing agent selected from the group consisting of a dye and a crease-resistance resin to a textile which comprises applying to the textile a solution, or a dispersion, or an emulsion of the finishing agent in a halogenated hydrocarbon solvent and then applying steam to the textile for a time sufficient to remove a major portion of the solvent, and immediately applying to the textile vapour of the said solvent at a temperature equal to or greater than the boiling point of the solvent.

2. A process as claimed in claim 1 wherein the textile material is an unmade-up textile.

3. A process as claimed in claim 1 wherein the said solvent comprises a chlorinated hydrocarbon solvent.

4. A process as claimed in claim 3 wherein the chlorinated hydrocarbon solvent is trichloroethylene or perchloroethylene.

5. A process as claimed in claim 1 wherein the textile is finally treated with solvent vapour at a temperature of at least 120 C.

6. A process as claimed in claim 5 wherein the temperature is not greater than 200 C.

7. A process as claimed in claim 5 wherein the temperature is from'l30 to 160 C.

30 seconds to 5 minutes. 

2. A process as claimed in claim 1 wherein the textile material is an unmade-up textile.
 3. A process as claimed in claim 1 wherein the said solvent comprises a chlorinated hydrocarbon solvent.
 4. A process as claimed in claim 3 wherein the chlorinated hydrocarbon solvent is trichloroethylene or perchloroethylene.
 5. A process as claimed in claim 1 wherein the textile is finally treated with solvent vapour at a temperature of at least 120* C.
 6. A process as claimed in claim 5 wherein the temperature is not greater than 200* C.
 7. A process as claimed in claim 5 wherein the temperature is from 130* to 160* C.
 8. A process as claimed in claim 1 wherein the textile is finally treated in a treatment vessel provided with means to heat the solvent vapour therein.
 9. A process as claimed in claim 3 wherein the solvent is recovered.
 10. A process as claimed in claim 1 wherein the final treatment with solvent vapour is for a period of from 30 seconds to 5 minutes. 